National Institute of Standards & Technology

Certificate of Analysis
Standard Reference Material 2710a
Montana I Soil

Highly Elevated Trace Element Concentrations

This Standard Reference Material (SRM) is intended primarily for use in the analysis of soils, sediments, or other
materials of a similar matrix. One unit of SRM 2710a consists of 50 g of the dried, powdered soil, blended with
lead oxide.

Certified Values: The certified concentrations for 22 elements, expressed as mass fractions [1] on a dry-mass
basis, are provided in Table 1. Certified values are based on results obtained from critically evaluated independent
analytical techniques. A NIST certified value is a value for which NIST has the highest confidence in its accuracy
in that all known or suspected sources of bias have been investigated or taken into account [2].

Reference Values: The reference values for 13 constituents, expressed as mass fractions on a dry-mass basis, are
provided in Table 2. Ten reference values are based on results obtained from a single NIST analytical method, and
three are based on results form two NIST analytical methods. Reference values are non-certified values that are the
best estimate of the true value; however, the values do not meet NIST criteria for certification and are provided with
associated uncertainties that may not include all sources of uncertainty [2].

Information Values: The values for 13 elements are provided in Table 3 for information purposes only. These are
non-certified values with no uncertainty assessed. The information values included in this certificate are based on
results obtained from one NIST method.

Expiration of Certification: The certification of SRM 2710a is valid, within the measurement uncertainties
specified, until 1 January 2019, provided the SRM is handled in accordance with the instructions given in this
certificate (see Instructions for Use). This certification is nullified if the SRM is damaged, contaminated, or
otherwise modified.

Maintenance of SRM Certification: NIST will monitor this SRM over the period of its certification. If
substantive technical changes occur that affect the certification before the expiration of this certificate, NIST will
notify the purchaser. Registration (see attached sheet) will facilitate notification.

E.A. Mackey and R.R. Greenberg of the NIST Analytical Chemistry Division were responsible for coordination of
the technical measurements leading to certification.

Statistical analyses were performed by J.H. Yen of the NIST Statistical Engineering Division.

Support aspects involved in the issuance of this SRM were coordinated through the NIST Measurement Services
Division.

Stephen A. Wise, Chief

Analytical Chemistry Division

Gaithersburg, MD 20899 Robert L. Watters, Jr., Chief

Certificate Issue Date: 7 April 2009 Measurement Services Division

SRM 2710a Page 1 of 7

INSTRUCTIONS FOR USE

Sampling: The SRM should be thoroughly mixed by repeatedly inverting and rotating the bottle horizontally
before removing a test portion for analysis. A minimum mass of 250 mg (dry mass - see Instructions for Drying)
should be used for analytical determinations to be related to the mass fraction values in this Certificate of Analysis.

To obtain the certified values, sample preparation procedures should be designed to effect complete dissolution. If
volatile elements (i.e., arsenic, mercury, selenium) will be determined, precautions should be taken in the
dissolution of SRM 2710a to avoid volatilization losses.

Drying: To relate measurements to the certified, reference, and information values that are expressed on a dry-mass
basis, users should determine a drying correction at the time of each analysis. The recommended drying procedure
is oven drying for 2 h at 110 C. Note that analytical determination of volatile elements (i.e., arsenic, mercury,
selenium) should be determined on samples as received; separate samples should be dried as previously described to
obtain a correction factor for moisture. Correction for moisture must be made to the data for volatile elements
before comparing to the certified values. This procedure ensures that these elements are not lost during drying. The
mass loss on drying for this material as bottled was approximately 2 %, but this value may change once the bottle is
opened and the soil is exposed to air.

SOURCE, PREPARATION, AND ANALYSIS

Source and Preparation of Material1: The U.S. Geological Survey (USGS), under contract to NIST, collected
and processed the material for SRM 2710a. The original collection site used for SRM 2710 was no longer available
due to remediation efforts by the Montana Department of Environmental Quality. An alternative nearby site,
located within the flood plain of the Silver Bow Creek, was selected. The site is approximately five miles west of
Butte, Montana. Soil for SRM 2710a was placed in 22 plastic-lined five-gallon buckets using a common garden
spade. The buckets were sealed and transferred to the USGS using a commercial freight carrier. At the USGS, the
SRM 2710a soil was dried at room temperature, disaggregated, and sieved to remove coarse material (2 mm). The
resulting soil was ball-milled in 50 kg portions together with an amount of lead oxide sufficient to achieve a mass
fraction of 0.55 % lead in the final product. The entire ball-milled batch of soil was transferred to a cross-flow
V-blender for mixing. The blended soil was radiation sterilized prior to bottling. In the final preparation step the
blended material was split into containers using a custom-designed spinning riffler, which was used to divide the
material into smaller batches, and then used to apportion approximately 50 g into each pre-cleaned bottle.

Every 100th bottle was set aside for chemical analyses designed to assess material homogeneity using X-ray
fluorescence spectrometry (XRF), inductively coupled plasma optical emission spectrometry (ICP-OES), and
inductively coupled plasma mass spectrometry (ICP-MS) at the USGS. Homogeneity assessments were performed
at NIST as well, and results indicated that additional processing was needed to achieve optimum homogeneity. The
material from all bottles was combined, and then ground in batches between stainless steel plates for a time
sufficient to produce a powder of which 95 %, by mass, passed through a 200 mesh (74 m) sieve. The resulting
powder was blended, and 50 g portions were dispensed into bottles using the spinning riffler. Results from
additional analyses indicated material homogeneity was acceptable (see below).

Analysis: The homogeneity was assessed for selected elements in the bottled material using X-ray fluorescence
spectrometry and instrumental neutron activation analysis (INAA). The estimated relative standard deviation for
material inhomogeneity is <1 % and no component for inhomogeneity was included in the expanded uncertainties of
the certified or reference values.

Analyses of this material were performed at NIST and at the USGS (Denver, CO). Results from NIST were used to
provide the certified, reference, and information values shown in Tables 1, 2, and 3 respectively. Results from the
USGS were used to confirm those values. The analytical techniques used for each element are listed in Table 4; the
analysts are listed in Tables 5 and 6.

1
Certain commercial equipment, instruments, or materials are identified in this certificate in order to specify
adequately the experimental procedure. Such identification does not imply recommendation or endorsement by the National
Institute of Standards and Technology, nor does it imply that the materials or equipment identified are necessarily the best
available for the purpose.

SRM 2710a Page 2 of 7

 (a,b)
Table 1. Certified Values (Dry-Mass Basis) for Selected Elements in SRM 2710a

Element Mass Fraction Element Mass Fraction

(%) (mg/kg)

Aluminum 5.95 0.05 Antimony 52.5 1.6

Arsenic 0.154 0.010 Barium 792 36
Calcium 0.964 0.045 Cadmium 12.3 0.3
Copper 0.342 0.005 Cobalt 5.99 0.14
Iron 4.32 0.08 Lanthanum 30.6 1.2
Lead 0.552 0.003 Mercury 9.88 0.21
Magnesium 0.734 0.038 Strontium 255 7
Manganese 0.214 0.006 Uranium 9.11 0.30
Phosphorus 0.105 0.004
Potassium 2.17 0.13
Silicon 31.1 0.4
Sodium 0.894 0.019
Titanium 0.311 0.007
Zinc 0.418 0.015

(a)
Certified values for all elements except lead and mercury are the equally weighted means of results from two or
three analytical methods. The uncertainty listed with each value is an expanded uncertainty about the mean. The
expanded uncertainty is calculated as U = kuc, where uc is intended to represent, at the level of one standard
deviation, the combined effect of between-method and within-method components of uncertainty, following the ISO
Guide [3,4]. The coverage factor (k) is determined from the Student's t-distribution corresponding to the
appropriate associated degrees of freedom and approximately 95 % confidence for each analyte.
(b)
The certified values for lead and mercury are each results from a single NIST method (see Table 4) for which a
complete evaluation of all sources of uncertainty has been performed. The uncertainties for the certified values for
these elements represent expanded uncertainties with a coverage factor of 2, with uncertainty components combined
following the ISO Guide [4].

SRM 2710a Page 3 of 7

 (a,b,c)
Table 2. Reference Values (Dry-Mass Basis) for Selected Elements in SRM 2710a

Element Mass Fraction (mg/kg)

Cesium 8.25 0.11

Chromium 23 6
Europium 0.82 0.01
Gadolinium 3.0 0.1
Lutetium 0.31 0.01
Neodymium 22 2
Nickel 8 1
Rubidium 117 3
Samarium 4.0 0.2
Scandium 9.9 0.1
Thallium 1.52 0.02
Thorium 18.1 0.3
Vanadium 82 9

(a)
Reference values for all elements except chromium, nickel, samarium, and vanadium are based on results
from one analytical method at NIST (see Table 4) and the uncertainties represent the expanded uncertainties,
which include the combined Type A and Type B with a coverage factor of 2, following the ISO Guide [4].
(b)
Reference values for nickel and samarium are the equally weighted means of results from two analytical
methods for nickel and two INAA experiments for samarium. The uncertainty listed with each value is an
expanded uncertainty about the mean. The expanded uncertainty is calculated as U = kuc, where uc is intended
to represent, at the level of one standard deviation, the combined effect of between-method and within-method
components of uncertainty, following the ISO Guide [3,4]. The coverage factor (k) is determined from the
Student's t-distribution corresponding to the appropriate associated degrees of freedom and approximately 95 %
confidence for each analyte.
(c)
Reference values for chromium and vanadium are based on a weighted mean calculated based on the
Dersimonian-Laird method [5], which incorporates an estimate of the between-method variance into the
weights. The expanded uncertainty listed with these values is calculated as U = kuc, where k = 2, and uc is
intended to represent, at the level of one standard deviation, the combined effect of between-method and
within-method components of uncertainty.

SRM 2710a Page 4 of 7

 (a)
Table 3. Information Values (Dry-Mass Basis) for Selected Elements in SRM 2710a

Element Mass Fraction (mg/kg)

Boron 20
Cerium 60
Dysprosium 3
Gold 0.2
Hafnium 7
Indium 7
Selenium 1
Silver 40
Tantalum 0.9
Terbium 0.5
Tungsten 190
Ytterbium 2
Zirconium 200

(a)
Information values are based on results from one analytical method at NIST

SRM 2710a Page 5 of 7

 Table 4. NIST Methods Used for the Analysis of SRM 2710a

Element Methods Element Methods

Ag INAA Na INAA; XRF

Al INAA; XRF Nd INAA
As CCT-ICP-MS; INAA; XRF Ni ICP-MS; ICP-OES
Au INAA P ICP-OES; XRF
B PGAA Pb ID-ICP-MS
Ba INAA: XRF Rb INAA
Ca INAA; XRF Sb ICP-MS; INAA
Cd ID-ICP-MS; PGAA Sc INAA
Ce INAA Se CCT-ICP-MS
Co INAA; ICP-OES Si PGAA; XRF
Cr INAA; XRF Sm INAA(a)
Cs INAA Sr ICP-OES; XRF
Cu INAA; XRF Ta INAA
Dy INAA Tb INAA
Eu INAA Th INAA
Fe INAA; PGAA; XRF Ti PGAA; XRF
Gd PGAA Tl ICP-MS
Hf INAA U ICP-MS; INAA
Hg CV-ID-ICPMS V INAA; XRF
K INAA; PGAA; XRF W INAA
La INAA(a) Yb INAA
Lu INAA Zn INAA; XRF
Mg INAA; XRF Zr XRF
Mn INAA; PGAA; XRF

NIST Methods of Analysis

CCT-ICP-MS Collision cell inductively coupled plasma mass spectrometry

CV-ID-ICP-MS Cold vapor isotope dilution inductively coupled plasma mass spectrometry
ICP-MS Inductively coupled plasma mass spectrometry
ICP-OES Inductively coupled plasma optical emission spectrometry
ID-ICP-MS Isotope dilution inductively coupled plasma mass spectrometry
INAA Instrumental neutron activation analysis
PGAA Prompt gamma-ray activation analysis
XRF X-ray fluorescence spectrometry

USGS Methods of Analysis(b)

WD-XRF-2 Wavelength dispersive X-ray fluorescence spectrometry at USGS

ICP-OES-2 Inductively coupled plasma optical emission spectrometry at USGS
ICP-MS-2 Inductively coupled plasma mass spectrometry at USGS
(a)
Two different INAA experiments, performed using different sub-samples and different analytical conditions, were
used to provide certified and reference values for lanthanum and samarium, respectively.
(b)
USGS Methods of Analysis were used to confirm results from certification methods.

SRM 2710a Page 6 of 7

 Table 5. Participating NIST Analysts:

S.J. Christopher S.A. Rabb

R.D. Day J.R. Sieber
S.E. Long R.O. Spatz
E.A. Mackey R.S. Popelka-Filcoff
A.F. Marlow B.E. Tomlin
J.L. Molloy L.J. Wood
K.E. Murphy L.L. Yu
R.L. Paul R. Zeisler

Table 6. Participating USGS Laboratory and Analysts

Laboratory Analysts

U.S. Geological Survey M.G. Adams

Branch of Geochemistry Z.A. Brown
Denver, CO, USA P.L. Lamothe
J.E. Taggart
S.A. Wilson

REFERENCES

[1] Thompson, A.; Taylor, B.N.; Guide for the Use of the International System of Units (SI), NIST Special
Publication 811 (2008); available at http://www.physics.nist.gov/Pubs/contents.html.
[2] May, W.E.; Gills, T.E.; Parris, R.; Beck, II, C.M.; Fassett, J.D.; Gettings, R.J.; Greenberg, R.R.; Guenther,
F.R.; Kramer, G.; MacDonald, B.S.; Wise, S.A.; Definitions of Terms and Modes Used at NIST for Value-
Assignment of Reference Materials for Chemical Measurements, NIST Special Publication 260-136
(1999); available at http://www.cstl.nist.gov/nist839/NIST_special_publications.htm.
[3] Levenson, M.S.; Banks, D.L.; Eberhardt, K.R.; Gill, L.M.; Guthrie, W.F.; Liu, H.K.; Vangel, M.G.; Yen,
J.H.; Zhang, N.F.; J. Res. NIST 105, pp. 571-579 (2000).
[4] ISO; Guide to the Expression of Uncertainty in Measurement, ISBN 92-67-10188-9, 1st ed.; International
Organization for Standardization: Geneva, Switzerland (1993); see also Taylor, B.N.; Kuyatt, C.E.;
Guidelines for Evaluating and Expressing the Uncertainty of NIST Measurement Results, NIST Technical
Note 1297, U.S. Government Printing Office, Washington, DC (1994); available at
http://www.physics.nist.gov/Pubs/contents.html.
[5] DerSimonian, R.; Laird, N.; Controlled Clinical Trials 7, 177-188 (1986).

Users of this SRM should ensure that the certificate in their possession is current. This can be accomplished by
contacting the SRM Program at: telephone (301) 975-2200; fax (301) 926-4751; e-mail srminfo@nist.gov; or via
the Internet at http://www.nist.gov/srm.

SRM 2710a Page 7 of 7

 Addendum to Certificate
Standard Reference Material 2710a
Montana I Soil

Highly Elevated Trace Element Concentrations

Leachable Concentrations Determined Using USEPA Methods 200.7 and 3050B

The mass fraction values contained in the NIST Certificate of Analysis for SRM 2710a represent the total element
content of the material. The measurement results used to provide the certified, reference or information values are
obtained from methods that require complete sample decomposition, or from nondestructive analytical methods
such as instrumental neutron activation analysis or prompt gamma-ray activation analysis. Where complete sample
decomposition is required, it can be accomplished by digestion with mixed acids or by fusion. For mixed-acid
decomposition, hydrofluoric acid must be included in the acid mixture used to totally decompose siliceous materials
such as soils and sediments.

In its monitoring programs, the U.S. Environmental Protection Agency (USEPA) has established a number of leach
methods for the preparation of soil samples for the determination of extractable elements. Six laboratories
participated, five of which used USEPA Method 200.7; the remaining laboratory used USEPA SW-846 Method
3050B for preparation of soil samples. All elements were determined in leachates by inductively coupled plasma
optical emission spectrometry. All laboratories provided individual results from duplicate portions, and these
results were averaged together to provide one result for each element from each participating laboratory. Results
rejected as outliers by the USEPA Contract Laboratory Program (CLP) officials were not included. Results are
summarized in Table A1. The ranges of mass fraction values, median values (to two significant figures), and the
number of results included for each are given for 23 elements. The percent recovery values based on the ratios of
the median values to the total element content (from the certified, reference, or information values in the Certificate
of Analysis) are listed in the last column of Table A1. Note that the certified values provided as total mass
fractions in the Certificate of Analysis are the best estimate of the true mass fraction values for this material.

This USEPA CLP Study was coordinated by Clifton Jones, Quality Assurance and Technical Support Program
(QATS), Shaw Environmental & Infrastructure Group, Las Vegas, NV, under the direction of John Nebelsick,
USEPA, Analytical Services Branch. The participating laboratories are listed in Table A2.

SRM 2710a Page 1 of 2

 Table A1. Results from Laboratories Participating in the EPA Contract Laboratory Program Study.

Element n Range (mg/kg) Median (mg/kg) Recovery (%)

Aluminum 6 8200 - 12000 10000 17
Antimony 6 5.0 - 12 9.6 18
Arsenic 6 1300 - 1600 1400 92
Barium 6 490 - 540 510 65
Beryllium 6 0.24 - 0.51 0.48 --
Cadmium 5 9.6 - 12 11 86
Calcium 6 1700 - 2000 1800 19
Chromium 6 9.2 - 11 10 41
Cobalt 6 2.8 - 5.2 3.8 64
Copper 6 3100 - 3500 3300 95
Iron 6 30000 - 36000 34000 79
Lead 6 4700 - 5800 5100 93
Magnesium 6 3200 - 3600 3500 48
Manganese 6 1500 - 1800 1700 77
Mercury 6 9.3 - 11.7 10 104
Nickel 5 4.8 - 6.1 5.5 69
Potassium 6 3800 - 4700 4100 19
Selenium 2 1.5 - 2.6 2.0 200
Silver 6 31 - 39 36 91
Sodium 6 550 - 650 590 7
Thallium 3 1.3 - 3.6 3.2 213
Vanadium 6 35 - 43 38 48
Zinc 6 3300 - 4400 3800 90

Table A2. List of CLP and non-CLP Participating Laboratories

A4 Scientific, Inc.
Bonner Analytical Testing Co.
Chem Tech Consulting Group
Datachem Laboratories, Inc.
Liberty Analytical Corporation
SVL Analytical, Inc.

SRM 2710a Page 2 of 2